CN104437433B - A kind of preparation method of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride base anionic dye adsorbent - Google Patents
A kind of preparation method of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride base anionic dye adsorbent Download PDFInfo
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- CN104437433B CN104437433B CN201410701612.3A CN201410701612A CN104437433B CN 104437433 B CN104437433 B CN 104437433B CN 201410701612 A CN201410701612 A CN 201410701612A CN 104437433 B CN104437433 B CN 104437433B
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- ammonium chloride
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
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Abstract
The invention provides a kind of preparation method of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride base anionic dye adsorbent, technical field of composite materials is set.With acrylamide, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride as polymerized monomer, palygorskite is inorganic filler to the present invention, is obtained by radical polymerization under conditions of crosslinking agent and initiator are present.The present invention adjusts formation and its spacial framework of polymer by the special construction on palygorskite surface, so as to increase the gap between effective binding molecule, improves absorption property.Experiment shows that adsorbent prepared by the present invention has good absorption property to anionic dye.
Description
The invention belongs to technical field of sewage, it is related to a kind of anionic dye adsorbent, more particularly to a kind of methyl
The preparation method of acrylyl oxy-ethyl-trimethyl salmiac base anionic dye adsorbent.
Background technology
Anionic dye waste water be at present it is very common be also very intractable class industrial wastewater, because its colourity is high, poison
Property the factor such as big, biodegradable and decolouring difficulty presence, the treatment of waste water from dyestuff always be difficult point in terms of water process with
Focus.The main method of dye wastewater treatment includes membrane filter method, and the precipitation method, freezing method, electrochemical process, ion-exchange is changed
Oxidizing process is learned, absorption method, wherein absorption method are because water quality is good and stabilization is especially subject in these all of methods after its treatment
Concern.
Compound adsorbent be it is a kind of with economic and environment-friendly, adsorption efficiency it is high, have the adsorbent of labyrinth, in water process
It is used widely.Chinese invention patent（CN 103508534 A）A kind of modified activated carbon waste water flocculant is disclosed, is used
Acrylic acid, acrylic amine, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride are modified to activated carbon, can be to water pollutant
Play more preferable flocculation reaction.But the raw material involved by the method for modifying is more, complex process, adsorbent does not form a list
One entirety, easily brings secondary pollution to water quality, and adsorption capacity is poor, it is impossible to application well.
The content of the invention
It is an object of the invention to provide a kind of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride base anionic dye adsorbent
Preparation method.
First, the preparation of anionic dye adsorbent
The present invention with acrylamide, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride as polymerized monomer, with palygorskite
It is, without tassement polaire, to be obtained by radical polymerization under conditions of crosslinking agent and initiator are present.Specifically preparation technology is：First will
In deionized water, the palygorskite ultrasonic disperse for adding acidified treatment is uniform, Ran Houjia for acrylic amine dispersed with stirring
Enter MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, crosslinking agent N, N'- methylene-bisacrylamide stirs 10 ~ 30 min, then to
Initiator is added in system, 50 ~ 75 DEG C of 0.5 ~ 2h of polymerisation are warming up to；Polymerizate through with absolute ethanol washing to neutrality,
Dry, crush, grind, cross 90 ~ 160 mesh sieves and obtain final product.
MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride is the principal monomer of polymer, and acrylamide causes methacryl
Oxy-ethyl-trimethyl salmiac monomer can aggregate into chain.Excessive polymerized monomer causes that the degree of polymerization of polymerizate is too high,
Contained adsorption site is wrapped in the composite of synthesis, so that the absorption property of composite has slightly declined.
The present invention determines that monomeric acrylamide is 1 with the mass ratio of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride by many experiments:
1~1:3。
Deionized water is the medium of monomer polymerization, and deionized water is not enough or the excessive polymerization for being all unfavorable for monomer：Deionization
Water is not enough so that the polymerization of monomer is insufficient；Deionized water excessively causes that the polymerization amount of monomer declines.Present invention determine that acrylic acid
Amine is 1.5 ~ 2.5g/ml with the mass volume ratio of deionized water, most beneficial for the polymerization of monomer.
Palygorskite can regulate and control network structure in the composition polymer of formation so that wherein contain as filler
Exposed more in activated adoption site.But palygorskite excess, can cause polymerizate degree of cross linking step-down, so as to reduce it
Absorption property.The present invention is by many experiments, it is determined that the palygorskite of acidification and methylacryoyloxyethyl front three
The mass ratio of ammonium chloride is 1:10~1:25.
The introducing of crosslinking agent can strengthen the polymerizing power of polymerized monomer.But the consumption of crosslinking agent is very few so that polymerization is short
Chain can not be connected effectively, so that polymerization is incomplete；The consumption of crosslinking agent is excessive, and can make the polymer of generation has more
Crosslinking points, so as to cause extra network cross-linked to be formed, so as to reduce the site space of absorption.This hair by many experiments, really
It is 1 to determine crosslinking agent N, N'- methylene-bisacrylamide with the mass ratio of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride:45~1:
60。
Initiator uses potassium peroxydisulfate, ammonium persulfate.The matter of initiator and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride
Amount is than being 1:80~1:100.
2nd, the structural analysis of anionic dye adsorbent
1st, infrared (FT-IR) spectrum analysis of Fourier
Fig. 1 is adsorbent prepared by the present invention（PADP）And palygorskite clay（PGS）Infrared spectrogram.3548cm-1,
3416cm-1, 3615cm-1It is the stretching vibration of palygorskite surface hydroxyl, 2934 cm-1It is the asymmetric stretching vibration peak of c h bond,
Corresponding 517cm-1And 470cm-1, 1029cm-1Left and right is the stretching vibration of Si-O keys.What these Si-O vibrated fades away
It is probably they are due to overall relative usage is reduced in modifying process.Another significant change is-OH peaks
Fade away, this is probably due to forming hydrogen bond between organic matter and palygorskite in compound adsorbent.
2nd, ESEM (SEM) analysis
Fig. 2 is palygorskite raw ore（PGS）The palygorskite of A, acidification（PGS）B and anionic dye adsorbent（PADP）C
Scanning electron microscope (SEM) photograph.A can be seen that palygorskite into bar-shaped and sheet, and the aggregation of substantial amounts of bar-shaped and sheet from the graph
Overlap together；The acidified palygorskite surface gap for obtaining is can be seen that from figure B to significantly increase, surface is loose, has
Abundant specific surface area；The polymer surfaces that introducing palygorskite is can be seen that by scheming C become smooth, and polymeric chain is deposited on
Between the surface and gap of palygorskite, in the spacial framework of amorphous state, this is reduced mainly due to the addition of clay
Crystallinity so that each ion is in homogeneous dispersion.And polymerized monomer, by polymerisation, the organo-functional group of monomer and slope are in detail
Interaction force is formed between the surface hydroxyl of stone clay, polymerization side chain and substantial amounts of organo-functional group are coated on palygorskite
Surface makes clay surface form polymer covering.Importantly, composite prepared by the present invention belongs to polymer mesh
Structure, after adding palygorskite so that the adsorption site of network polymers increases, and improves its adsorption capacity；Simultaneously because palygorskite
Clay absorption property in itself further enhancing the absorption property of composite；In addition, palygorskite increase effectively absorption
Intermolecular gap, improves the absorption property of material.
3rd, absorption property of the adsorbent to anionic dye
By taking anionic dye methyl orange as an example：Configuration concentration is the methyl orange standard liquid of 100 mg/L, takes 50 mL molten
The conical flask for being added to wash clean of liquid（There-necked flask）In, conical flask is positioned in constant temperature oscillation bed, weigh prepared
Composite adsorbing material 0.01g is added thereto, and is sealed with preservative film, and temperature is 25 DEG C, and the concussion time is 2.5h, and concussion speed is
160rpm, stands 5min.Its supernatant is taken, the concentration of wherein methyl orange dye is determined with ultraviolet specrophotometer, by initial dense
Degree can be calculated the adsorbance of the adsorbent with the residual quantity of ultimate density.
Experimental result：Adsorbance to methyl orange dye is up to 833mg/g, and clearance can be up to 97.3%.
It is fine that similar experiment is also shown that adsorbent prepared by the present invention also has to for example Congo red grade of other anionic dyes
Absorption property：, in 486.5 more than mg/g, clearance is more than 95% for adsorbance.
Brief description of the drawings
Fig. 1 is adsorbent prepared by the present invention（PADP）And palygorskite clay（PGS）Infrared spectrogram.
Fig. 2 is palygorskite raw ore（PGS）The palygorskite of A, acidification（PGS ）B and anionic dye adsorbent（PADP）
The scanning electron microscope (SEM) photograph of C.
Specific embodiment
Make into one below by preparation of the specific embodiment to sorbing material of the present invention and its absorption property to anion
Step explanation.
Embodiment one
1st, the acidification of palygorskite：A certain amount of palygorskite raw ore is added in 1000 mL beakers, plus
Water is to 600 mL, mechanical agitation（1000 rpm）8 h.Gained suspension dilute with water, after standing a period of time, topples over upper strata clear
Liquid and bottom sand bed, after mud suspension in intermediate layer is washed into three times, drying is crushed, in being acidified and be washed to 1 M hydrochloric acid
Property, dry, crush, cross 200 mesh sieves, the palygorskite being acidified（PGS）.
2nd, the preparation of compound adsorbent：Take 7.5 g acrylic amines（AM）It is added in there-necked flask with 5 ml deionized waters,
At room temperature with after the min of mechanical agitation 10, the PGS of 0.75 g is added, quickly stir ultrasonic 30 min；It is slowly added dropwise 7.5 g first
Base acrylyl oxy-ethyl-trimethyl salmiac（DMC）Into system, and add 0.167 g crosslinking agents N, N'- di-2-ethylhexylphosphine oxide third
Acrylamide（MBA）, continue to stir 30 min, add 0.09375 g initiator potassium persulfates（KPS）, 75 DEG C are warming up to, slowly
Stirring to polymer is formed, and stops stirring, continues to react 2 h.Product uses absolute ethanol washing three times after shredding（To neutrality）,
And in 75 DEG C of dryings to constant weight, product is by crushing, grinding, crosses 90-160 mesh sieves, dries.
3rd, to Anion-adsorption performance:After testing, the adsorbent is 827mg/g, clearance to the adsorption capacity of methyl orange
It is 96 %；It is 412 mg/g, clearance 91% to Congo red adsorption capacity.
Embodiment 2
1st, with example 1.
2nd, the preparation of compound adsorbent：Take 7.5 g acrylic amines（AM）It is added in there-necked flask with 3 ml deionized waters,
At room temperature with after the min of mechanical agitation 10, the PGS of 0.3 g is added, quickly stir ultrasonic 30 min；It is slowly added dropwise 7.5 g first
Base acrylyl oxy-ethyl-trimethyl salmiac（DMC）Into system, and add 0.125 g crosslinking agents N, N'- di-2-ethylhexylphosphine oxide third
Acrylamide（MBA）, continue to stir 30 min, 0.075 g initiator ammonium persulfates are added, 75 DEG C are warming up to, it is slowly stirred to poly-
Compound is formed, and stops stirring, continues to react 2 h.Product uses absolute ethanol washing three times after shredding（To neutrality）, and 75
, to constant weight, product is by crushing, grinding, crosses 90-160 mesh sieves, dries for DEG C drying.
3rd, to Anion-adsorption performance:After testing, the adsorbent is 833 mg/g, clearance to the adsorption capacity of methyl orange
It is 97.3 %；It is 486.5 mg/g, clearance 95.1% to Congo red adsorption capacity.
Embodiment 3
1st, with example 1.
2nd, the preparation of compound adsorbent：Take 7.5 g acrylic amines（AM）It is added in there-necked flask with 5 ml deionized waters,
At room temperature with after the min of mechanical agitation 10, the PGS of 2.25 g is added, quickly stir ultrasonic 30 min；It is slowly added dropwise 22.5 g
MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride（DMC）Into system, and add 0.5 g crosslinking agents N, N'- di-2-ethylhexylphosphine oxide third
Acrylamide（MBA）, continue stir 30 min, add 0.28125 g initiator ammonium persulfates, be warming up to 75 DEG C, be slowly stirred to
Polymer is formed, and stops stirring, continues to react 2 h.Product uses absolute ethanol washing three times after shredding（To neutrality）, and 75
, to constant weight, product is by crushing, grinding, crosses 90-160 mesh sieves, dries for DEG C drying.
3rd, to Anion-adsorption performance:After testing, the adsorbent is 801 mg/g, clearance to the adsorption capacity of methyl orange
It is 93 %；It is 414.5 mg/g, clearance 90% to Congo red adsorption capacity.
Embodiment 4
1st, with example 1.
2nd, the preparation of compound adsorbent：Take 7.5 g acrylic amines（AM）It is added in there-necked flask with 3 ml deionized waters,
At room temperature with after the min of mechanical agitation 10, the PGS of 0.9 g is added, quickly stir ultrasonic 30 min；It is slowly added dropwise 22.5 g first
Base acrylyl oxy-ethyl-trimethyl salmiac（DMC）Into system, and add 0.375 g crosslinking agents N, N'- di-2-ethylhexylphosphine oxide third
Acrylamide（MBA）, continue to stir 30 min, 0.225 g initiator potassium persulfates are added, 75 DEG C are warming up to, it is slowly stirred to poly-
Compound is formed, and stops stirring, continues to react 2 h.Product uses absolute ethanol washing three times after shredding（To neutrality）, and 75
, to constant weight, product is by crushing, grinding, crosses 90-160 mesh sieves, dries for DEG C drying.
3rd, to Anion-adsorption performance:After testing, the adsorbent is 812 mg/g, clearance to the adsorption capacity of methyl orange
It is 91 %；It is 402 mg/g, the % of clearance 89 to Congo red adsorption capacity.
Claims (2)
1. a kind of preparation method of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride base anionic dye adsorbent, is with acryloyl
Amine, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride are polymerized monomer, and palygorskite is inorganic filler, in crosslinking agent and initiation
Agent is obtained under conditions of existing by radical polymerization；Its specific preparation technology is：First by acrylamide dispersed with stirring in go from
In sub- water, the palygorskite ultrasonic disperse for adding acidified treatment is uniform, is subsequently adding methylacryoyloxyethyl front three
Ammonium chloride, crosslinking agent N, N'- methylene-bisacrylamide stirs 10 ~ 30 min, then to initiator is added in system, heat up
To 50 ~ 75 DEG C of 0.5 ~ 2h of polymerisation；Polymerizate is through with absolute ethanol washing to neutrality, drying, crushing, grinding, cross 90 ~
160 mesh sieves are obtained final product；
Monomeric acrylamide is 1 with the mass ratio of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride: 1~1:3；Acidified treatment
Palygorskite is 1 with the mass ratio of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride:10~1:25；
Initiator is potassium peroxydisulfate, ammonium persulfate；Initiator is with the mass ratio of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride
1:80~1:100；
Crosslinking agent N, N'- methylene-bisacrylamide is 1 with the mass ratio of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride:45~
1:60。
2. the preparation side of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride base anionic dye adsorbent as claimed in claim 1
Method, it is characterised in that：Acrylamide is 1.5 ~ 2.5g/mL with the mass volume ratio of deionized water.
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| CN108341906B (en) * | 2018-03-12 | 2020-03-17 | 福州大学 | Preparation method and application of cationic dye composite adsorption material |
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| CN110746652B (en) * | 2019-10-25 | 2020-12-08 | 安徽江淮汽车集团股份有限公司 | Preparation method of polyolefin VOC (volatile organic compound) improved filler and polyolefin composite material |
| CN117003939A (en) * | 2023-08-11 | 2023-11-07 | 中国铁工投资建设集团有限公司 | Weak alkaline gel ion exchange resin for adsorbing hexavalent chromium and preparation method thereof |
| CN117861621A (en) * | 2024-01-24 | 2024-04-12 | 安徽科凌沃特水处理技术有限公司 | Biochar/polyaluminum chloride composite adsorbent |
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